Fish Sampling and Analysis for PFOS

in Largemouth Bass from the

Tennessee River in the Vicinity

of the 3M Decatur Facility 

3M Company

Decatur, Alabama 

May 2012

11P-0094-7

3M Company

St. Paul, Minnesota

®
FISH SAMPLING AND ANALYSIS FOR PFOS 

IN LARGEMOUTH BASS 

 FROM THE TENNESSEE RIVER 

IN THE VICINITY OF THE 

3M DECATUR FACILITY, DECATUR, ALABAMA

May 2012 

Prepared for 

3M Company 

St. Paul, MN 

by 

WESTON SOLUTIONS, INC. 

West Chester, PA 19380 

W.O. No. 02181.129.122 
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TABLE OF CONTENTS 

Section Page 

1. INTRODUCTION.......................................................................................................... 1-1

2. MATERIALS AND METHODS .................................................................................. 2-1

3. RESULTS ....................................................................................................................... 3-1

4. REFERENCES ............................................................................................................... 4-1

APPENDICES 

APPENDIX A 3M ENVIROMENTAL LABORATORY 

 ANALYTICAL DATA PACKAGES 

APPENDIX B AXYS LABORATORY 

 ANALYTICAL DATA PACKAGE 
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LIST OF TABLES 

Section Page 

Table 3-1 Fish Sampling Summary and Catch Per Unit Effort ............................................ 3-8

Table 3-2 Fish Morphometrics and PFOS Concentrations .................................................. 3-9

Table 3-3 Largemouth Bass Filet PFOS Concentration Summary Statistics ..................... 3-10

Table 3-4 Surface Water PFOS Concentrations-April 2012 .............................................. 3-11
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LIST OF FIGURES 

Section Page 

Figure 2-1 Fish and Surface Water Sampling Locations-April 2012 .................................... 2-4

Figure 3-1 Largemouth Bass Filet PFOS Concentrations-April 2012................................... 3-4

Figure 3-2 Largemouth Bass Filet PFOS Concentration Box and Dot Plots ........................ 3-5

Figure 3-3 Largemouth Bass Filet PFOS Concentrations vs. Length ................................... 3-6

Figure 3-4 Surface Water PFOS Concentrations-April 2012 ................................................ 3-7
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1. INTRODUCTION 

Fish sampling was performed at three adjoining reaches spanning a distance of 2.5 miles 

in the Tennessee River in the vicinity of the 3M facility in Decatur, Alabama from April 

3 through 6, 2012 to characterize current concentrations of perfluorooctanesulfonate 

(PFOS) in filet samples from largemouth bass (Micropterus salmoides). The largemouth 

bass was selected for sampling for the following reasons: 

• Correspondence with the fish samples collected in earlier sampling performed by 

3M in 2004 and 2006 and subsequent collections by the Alabama Department of 

Environmental Management (ADEM) in 2007, 2008 and 2009; 

• Predator species representing the highest trophic level; and 

• Recommended target species (EPA, 1993; EPA 2000). 

In addition to collecting fish samples, surface water samples were collected from each 

fish sampling reach for PFOS analysis. Prior to sampling, a draft Work Plan for Fish 

Sampling and Analysis for PFOS in Largemouth Bass in the Tennessee River in the 

Vicinity of the 3M Decatur Facility (draft Work Plan) was prepared for review by the 

Alabama Department of Environmental Management (ADEM) and the Alabama 

Department of Public Health (ADPH). The Work Plan was subsequently revised to 

reflect comments received (WESTON, 2012). The following sections describe the 

sampling activities and provide the analytical results for PFOS concentrations in filet 

tissue and water samples. 
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2. MATERIALS AND METHODS 

A scientific collection permit (SCP) was obtained from the Alabama Department of 

Conservation and Natural Resources (DCNR) for fish collection. All collection efforts 

were performed in accordance with the SCP requirements including providing advance 

notification of pending field collection activities to the appropriate DCNR regional 

fisheries management/enforcement personnel. ADEM personnel were also notified and 

observed virtually the entire sample collection process. Electrofishing was conducted 

using a boat-mounted, generator-powered Smith-Root VI-A electrofisher fitted with two 

bow-mounted anodes and a single trailing cathode. 

Sampling reaches were shoreline lengths of approximately 0.75 miles. The upper reach was 

the southern shoreline of the Tennessee River above the confluence of Bakers Creek and 

extended to the east. The central reach was the shoreline within the mouth of Bakers Creek 

and the lower reach extended along the southern shoreline of the Tennessee River adjacent 

to the 3M property. The mouth of Bakers Creek and lower sampling reaches correspond 

respectively with the DBC and DOU collection locations in the 2004 and 2006 fish 

sampling activities performed by 3M (Weston 2008). The three fish sampling reaches are 

shown in Figure 2-1. Electrofishing focused on shoreline areas where sufficient structure 

exists to attract and hold largemouth bass. Based on input from the ADEM, the target size 

range for largemouth bass to be collected was 13-18 inches in length in an attempt to 

coincide with the size range of fish collected previously by ADEM. The target sample size 

of largemouth bass from each of the three fish sampling reaches was 10 fish for a total target 

of 30 fish specimens. Fish collection was performed under oversight by personnel from 

ADEM who were present in a separate boat. These individuals also observed sample 

preparation and other procedural aspects of the study. 

Surface water samples were collected using a peristaltic pump from each of the three 

sampling reaches during fish collection activities for PFOS analyses. Sampling depth was 

determined on the basis of total water depth. Because the surface water sampling locations 

were less than 10 feet deep, samples were collected at the 0.6 depth (six-tenths of the total 

depth of water measured from the surface). In addition to collecting surface water samples 
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for laboratory analysis of PFOS concentrations, routine water quality data including the 

parameters of temperature, specific conductance, dissolved oxygen, pH and turbidity were 

also collected at the sampling locations. 

In order to collect data suitable for assessing the range of variability in fish tissue PFOS 

concentrations and for consistency with past 3M and ADEM collections, samples were 

prepared from individual fish specimens for analysis rather than composite samples from 

multiple specimens. Sample IDs were assigned in the sequence of sample collection and 

did not contain information on the sampling locations. Each fish retained for tissue 

analysis was weighed and the total length was measured. Per input received from ADEM, 

skin-off filet tissue samples were prepared in the field from the right side filets of the fish 

specimens. In addition to the primary samples, field duplicate samples and quality 

assurance/quality control (QA/QC) samples were prepared. Field QA/QC samples 

included the collection of three equipment rinseate blanks to document the adequacy of 

decontamination of knives used to prepare the fish filet samples. Filet tissue samples 

were shipped frozen to the Michigan State University Wildlife Toxicology Laboratory 

(MSU WFL) for preparation of tissue homogenates. As instructed by the Study Director, 

MSU WTL forwarded the homogenized samples to the appropriate laboratories for 

analysis. The 3M Environmental Laboratory in St. Paul, Minnesota served as the primary 

laboratory for this study. The AXYS Analytical Services, Ltd. (AXYS) laboratory in 

Sidney, British Columbia, Canada, provided validation results in this study design. 

Field duplicate samples were prepared in the field from the left side filets of the chosen 

fish specimens. The left side filet was removed after the right side filet had been removed 

and was prepared as a skin-off filet tissue sample. Six left side skin-off fillets were 

chosen at random and sent as field duplicate samples to MSU WTL for preparation of 

tissue homogenates. Three of these duplicates were provided to the 3M Environmental 

Laboratory and the other three were sent to AXYS. The source of the blind field 

duplicates was not revealed to either laboratory. The blind field duplicates had unique 

sample identification numbers on the Chain of Custody form sent to the laboratory such 

that the laboratory could not determine its source. Additional left side filets collected and 
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not required for QA/QC analysis were prepared as skin-on filets, frozen and transferred to 

the 3M Environmental Laboratory to be retained indefinitely. 

Additionally, process control fish samples were sent by the 3M Environmental 

Laboratory to the MSU WTL to be analyzed before, during and after the processing of 

the field samples to confirm adequate decontamination of homogenization equipment 

between preparation of individual study samples and the absence of other contamination 

vectors associated with the preparation of the tissue homogenates. Following 

homogenization, these samples were returned to the 3M Environmental Laboratory for 

analysis. 

Finally, a standard reference material (SRM) fish tissue sample obtained from the 

National Institute of Standards and Technology (NIST) was sent to MSU WTL to be 

repackaged into two aliquots. One aliquot was forwarded to AXYS for analysis and the 

other aliquot was sent to the 3M Environmental Laboratory for analysis. 

The 3M Environmental Laboratory analyzed each tissue homogenate sample and a 

laboratory duplicate for PFOS. As noted above, three split samples prepared from skinoff left side filets (representing 10% of the target sample number collected) were also 

analyzed for PFOS by AXYS. Surface water samples were analyzed for PFOS by the 3M 

Environmental Laboratory. 
Tennesee River

3M Decatur

Lower Reach

Middle Reach

Upper Reach

LOC001

LOC002

LOC003

Flow

Bakers

Creek

0 500 1,000Feet

Legend:

3M Decatur, AL Facility

Figure 2-1

Fish and Surface Water 

Sampling Locations 

April 2012

Bakers Creek and

Tennessee River

File: Y:\3MDec\MXD\Fish_SW_Sampling_Locs.mxd, 5/1/2012 12:09:12 PM, ricksc

Imagery Source: ESRI Bing 

Mapping Service 2011

Fish Sampling Location

Surface Water 

Sampling Locations
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3. RESULTS 

A total of 26 largemouth bass were collected between the three sampling reaches during 

the week of April 2, 2012. Ten fish each were collected in the upper reach above the 

mouth of Bakers Creek and the middle reach at the mouth of Bakers Creek and six fish 

were collected from the lower reach below the mouth of Bakers Creek. A summary of the 

individual electrofishing runs including the overall elapsed times, the timer seconds 

recorded during which a potential was applied by the electrofishing unit, the number of 

bass captured and the catch per unit effort (CPUE) is provided in Table 3-1. Total time of 

collection varied by reach with the upper reach requiring approximately two hours and 

the middle reach requiring approximately 3.5 hours to obtain the target number of 10 fish 

specimens each. In contrast, a total of over 10 hours were expended to obtain the six fish 

specimens from the lower reach. On April 6, 2012, the last scheduled day for fish 

collection, efforts to collect additional specimens from the lower reach were suspended 

when winds of over 20 miles per hour from the north northeast prevented safe vessel 

operation along the lee shore. 

Fish lengths, weights and skin-off filet PFOS concentrations are tabulated by sampling 

reach in Table 3-2 and analytical results are shown in Figure 3-1. The analytical data 

packages for analyses performed by the 3M Environmental Laboratory are provided in 

Appendix A and the analytical data package for analyses of split samples performed by 

the AXYS laboratory is provided in Appendix B. While the majority of the fish were 

within ADEM’s target length range of 13 to 18 inches, one specimen from the middle 

reach slightly exceeded the target range (MSF13; 18.5 inches total length). One fish in 

the upper reach (MSF03; 12 inches total length) and three fish from the lower reach 

(MSF01, MSF16 and MSF22; 10.75, 12.5 and 11.25 inches total length, respectively) 

were below ADEM’s target range but above the 8 inch minimum length established in the 

original draft Work Plan. 

Comparisons of primary sample and field duplicate sample PFOS concentrations 

obtained from analysis by the 3M Environmental Laboratory indicated good 

correspondence with relative percent difference (RPD) values ranging from 2 to 9% for 
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the study fish. Comparisons of split sample PFOS concentrations obtained by the AXYS 

laboratory of left hand filets with the results from the 3M Environmental Laboratory 

analyses of the corresponding right hand filets indicated less, but acceptable, agreement 

with RPDs ranging from 21 to 33%. The AXYS PFOS concentrations were higher than 

the respective 3M Environmental Laboratory PFOS concentrations for the split samples. 

The AXYS analyses did not include analysis of PFOS laboratory matrix spike (LMS) 

sample(s) at sufficiently high concentrations relative to endogenous concentrations of 

PFOS for use in the evaluation of method performance. The 3M Environmental 

Laboratory analyzed PFOS LMS samples at relevant concentrations for each of the 

specimens and LMS recoveries ranged from 77% to 125%. (overall mean recovery ± 

standard deviation of 99% ± 10%). 

The overall comparison of PFOS concentrations measured in all fish samples indicated 

good agreement between laboratories. In general, PFOS concentrations reported by 

AXYS were greater than those from 3M for the samples. There was a systematic 

difference in the reported PFOS concentrations between both laboratories, but this is not 

unexpected given the potential difference in analytical methodologies used at each 

laboratory (Lindström et al. 2009). For instance, the use of linear isomer PFOS 

calibration with a 499 to 80 MS/MS transition for data acquisition by AXYS but not by 

the 3M Environmental Laboratory can bias high the quantification of mixed 

branched/linear PFOS in environmental samples by 8% (Riddell et al. 2009). Given what 

is known about the variability in the quantification of PFOS in biological tissues, results 

from this interlaboratory comparison reinforce the validity of the results of this study. 

Summary statistics for the largemouth bass filet tissue PFOS concentrations obtained by 

the 3M Environmental Laboratory analysis of primary (right hand filet) samples are 

provided in Table 3-3. Median largemouth bass filet tissue PFOS concentrations were 

624, 1930 and 979 ng/g for the upper, middle and lower reaches, respectively and 852 

ng/g for the combined data set (all reaches). Fish filet concentration data for each of the 

reaches is depicted in box plots (Figure 3-2). A scatter plot of PFOS and specimen length 

indicates no correlation between concentration and length (Figure 3-3). 
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3-3

Only one of three intended sets of water samples were collected. Collection of a second 

set was planned for April 6, 2012 but, as previously noted, unsafe conditions on the river 

precluded this action. The intended splitting of water samples with the AXYS laboratory 

did not occur, in part due to the accelerated pace of this study. Surface water PFOS 

concentrations and routine water quality parameters are tabulated in Table 3-4 and shown 

in Figure 3-2. 
Tennesee River

3M Decatur

Lower Reach

Middle Reach

Upper Reach

Flow

Bakers

Creek

LOC001

LOC002

LOC003

0 500 1,000Feet

Legend:

3M Decatur, AL Facility

Figure 3-1

Largemouth Bass Filet 

PFOS Concentrations 

April 2012

Bakers Creek and

Tennessee River

File: Y:\3MDec\MXD\Largemouth_Bass_PFOS_April2012.mxd, 5/9/2012 9:56:43 AM, ricksc

Imagery Source: ESRI Bing 

Mapping Service 2011

Fish Sampling Location

Surface Water 

Sampling Locations

Note: PFOS concentrations are

 the average of primary and 

 duplicate sample analytical 

 results on a wet weight basis.

Middle Reach PFOS (ng/g)

MSF02 4240

MSF07 2920

MSF08 1360

MSF09 2020

MSF27 (MSF09D) 2120

MSF10 1840

MSF11 2940

MSF11D (AXYS) 3720

MSF11D (AXYS Dup) 3510

MSF12 526

MSF13 950

MSF14 3370

MSF15 754

Lower Reach PFOS (ng/g)

MSF01 4770

MSF16 1520

MSF17 165

MSF28 (MSF17D) 180

MSF24 437

MSF24D (AXYS) 537

MSF25 306

MSF26 2090

MSF29 (MSF26D) 2050

Upper Reach PFOS (ng/g)

MSF03 70.7

MSF04 576

MSF05 471

MSF05D (AXYS) 656

MSF06 156

MSF18 701

MSF19 675

MSF20 1180

MSF21 671

MSF22 4660

MSF23 52.5
Figure 3-2 

Largemouth Bass Filet PFOS Concentration Box Plots 

0.0

1000.0

2000.0

3000.0

4000.0

5000.0

Combined Lower Middle Upper

Reach

PFOS (ng/g)

Whiskers (T) denote the largest (and smallest) adjacent values within 1.5 times the interquartile range (IQR) 

Red dot denotes an outlier greater than 1.5 times the IQR above the upper quartile (75th percentile) value
3000.0

4000.05000.0

PFOS (ng/g)

Figure 3‐3

Largemouth Bass PFOS Concentrations vs. Length

0.0

1000.02000.0

0.00 5.00 10.00 15.00 

Length (inches)
3M Decatur

Lower Reach

Middle Reach

Upper Reach

Tennesee River

Flow

Bakers

Creek

0 500 1,000Feet

Legend:

3M Decatur, AL Facility

Figure 3-4

Surface Water 

PFOS Concentrations 

April 2012

Bakers Creek and

Tennessee River

File: Y:\3MDec\MXD\Surface_Water_PFOS_April2012.mxd, 5/10/2012 10:45:30 AM, ricksc

Imagery Source: ESRI Bing 

Mapping Service 2011

Fish Sampling Location

Surface Water 

Sampling Locations

Note: PFOS concentrations are

 the average of primary and 

 duplicate sample analytical 

 results.

Sample ID PFOS (ng/mL)

LOC001 0.450

Sample ID PFOS (ng/mL)

LOC002 0.691

Sample ID PFOS (ng/mL)

LOC003 0.0237
Table 3-1

Fish Sampling Summary and Catch Per Unit Effort

Date Run Reach Hours

Timer 

(seconds)

Timer 

(hours)

Bass 

(count)

CPUE 

(bass/hour

4/3/2012 1 Lower 1.00 1355 0.38 1 1.00 4/3/2012 2 Middle 1.00 1680 0.47 1 1.00 4/3/2012 3 Upper 1.00 1939 0.54 4 4.00 4/3/2012 4 Middle 1.08 1897 0.53 9 8.31 4/4/2012 1 & 2 Lower 2.00 3459 0.96 2 1.00 4/4/2012 3 Upper 1.25 2253 0.63 2 1.60 4/4/2012 4 Upper 1.20 1112 0.31 4 3.33 4/4/2012 5 Lower 1.00 1809 0.50 0 0.00 4/4/2012 6 Lower 1.00 1525 0.42 0 0.00 4/5/2012 1 Lower 1.17 2071 0.58 1 0.86 4/5/2012 2 Lower 1.25 2020 0.56 0 0.00 4/5/2012 3 Lower 2.00 2806 0.78 1 0.50 4/6/2012 1 Lower 0.67 1291 0.36 1 1.50 Summary Total Total Hours

Total 

Timer 

(seconds)

Total 

Timer 

(hours)

Total 

Bass 

(count)

Average 

CPUE 

(bass/hour

Lower Reach 9 10.08 16336 4.54 6 0.61 Middle Reach 2 2.08 3577 1 10 4.65 Upper Reach 3 3.45 5304 1.47 10 2.98 Overall 14 15.62 25217 7.00 26 1.78 Notes:CPUE = Catch per unit effortTimer seconds record the number of seconds that the electrofisher potential was applied
Table 3-2

Fish Morphometrics and PFOS Concentrations

Sample ID Date Analytical Laboratory

Sampling 

Reach

Length 

(inches)

Weight 

(pounds)

PFOS 

MSF03 4/3/2012 3M Environmental Laboratory Upper 12.00 0.9 MSF04 4/3/2012 3M Environmental Laboratory Upper 14.75 1.7 MSF05 4/3/2012 3M Environmental Laboratory Upper 17.75 2.9 MSF05D 4/3/2012 AXYS Laboratory Upper " " MSF06 4/3/2012 3M Environmental Laboratory Upper 14.00 1.5 MSF18 4/4/2012 3M Environmental Laboratory Upper 15.75 2.5 MSF19 4/4/2012 3M Environmental Laboratory Upper 14.75 1.8 MSF20 4/4/2012 3M Environmental Laboratory Upper 14.25 1.0 MSF21 4/4/2012 3M Environmental Laboratory Upper 17.00 2.8 MSF22 4/4/2012 3M Environmental Laboratory Upper 11.25 0.8 MSF23 4/4/2012 3M Environmental Laboratory Upper 17.50 3.1 

MSF02 4/3/2012 3M Environmental Laboratory Middle 14.50 1.8 MSF07 4/3/2012 3M Environmental Laboratory Middle 16.00 2.2 MSF08 4/3/2012 3M Environmental Laboratory Middle 13.50 1.3 MSF09 4/3/2012 3M Environmental Laboratory Middle 13.25 1.2 MSF09D (MSF27) 4/3/2012 3M Environmental Laboratory Middle " " MSF10 4/3/2012 3M Environmental Laboratory Middle 14.00 1.7 MSF11 4/3/2012 3M Environmental Laboratory Middle 15.375 2.0 MSF11D 4/3/2012 AXYS Laboratory Middle " " MSF11D (Duplicate) 4/3/2012 AXYS Laboratory Middle " " MSF12 4/3/2012 3M Environmental Laboratory Middle 15.50 2.1 MSF13 4/3/2012 3M Environmental Laboratory Middle 18.50 3.3 MSF14 4/3/2012 3M Environmental Laboratory Middle 17.50 3.6 MSF15 4/3/2012 3M Environmental Laboratory Middle 17.50 3.3 

MSF01 4/3/2012 3M Environmental Laboratory Lower 10.75 0.5 MSF16 4/4/2012 3M Environmental Laboratory Lower 12.50 1.0 MSF17 4/4/2012 3M Environmental Laboratory Lower 13.75 1.2 MSF17D (MSF28) 4/4/2012 3M Environmental Laboratory Lower " " MSF24 4/5/2012 3M Environmental Laboratory Lower 16.00 2.1 MSF24D 4/5/2012 AXYS Laboratory Lower " " MSF25 4/5/2012 3M Environmental Laboratory Lower 16.50 2.1 MSF26 4/5/2012 3M Environmental Laboratory Lower 15.00 1.7 MSF26D (MSF29) 4/5/2012 3M Environmental Laboratory Lower " " 

Notes:PFOS concentrations are the average of the primary and duplicate analytical results expresssed in ng/g (ppb) on a weSample IDs with a "D" suffix are field duplicates obtained from left side filet samples
Table 3-3

Largemouth Bass PFOS Concentration Summary Statistics

Parameter Upper Reach Middle Reach Lower Reach Comb

Minimum 52.5 526 165 Maximum 4660 4240 4770 Mean 921 2092 1548 Median 624 1930 979 Geometric Mean 440 1725 833 Standard Deviation 1358 1238 1753 Notes:PFOS concentrations in ng/g (wet weight).Summary statistics obtained from primary data (field duplicate / split sample data not included).
Table 3-4

Surface Water Data

Lower Reach Middle Reach Upper Reach

Sample Station ID LOC001 LOC002 LOC003Northing (Decimal degrees) 34.644 34.638 34.637Westing (Decimal degrees) 87.035 87.029 87.021Date 04/05/12 04/05/12 04/05/12Time 9:50 10:17 10:37Temperature (°C) 21.63 21.77 21.5Specific conductance (μs/cm) 189 187 193Dissolved oxygen (mg/L) 7.74 9.75 8.13pH (S.U.) 7.33 8.13 7.56Turbidity (NTU) 35.2 23.5 21.5

Average PFOS (ng/mL) 0.450 0.691 0.0237

Notes:Average PFOS concentration is the average of primary and duplicate analytical results in ng/mL (ppb
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4. REFERENCES 

EPA. 2000. Guidance for Assessing Chemical Contaminant Data for Use in Fish 

Advisories, Volume I, Fish Sampling and Analysis. Third Addition. EPA. Office of 

Water. Washington, District of Columbia. 

EPA. 1993. Fish Field and Laboratory Methods for Evaluating the Biological Integrity of 

Surface Waters. EPA. Environmental Monitoring Systems Laboratory. Cincinnati, OH. 

Reynolds. J.B. 1996. Electrofishing. Pages 221-254 in B.R. Murphy and D.W. Willis 

editors. Fisheries Techniques, Second Edition. American Fisheries Society. Bethesda, 

MD. 

WESTON 2008. Perfluorinated Sulfonates Data Report, 3M Decatur, Alabama Facility, 

Site-Related Environmental Monitoring Program, September 2008, Weston Solutions, 

Inc., West Chester, PA. 

Lindström G., Karrman A., and van Bavel B. (2009). Accuracy and precision in the 

determination of perfluorinated chemicals in human blood verified by interlaboratory 

comparisons. J. Chromatogr. A 1216: 394-400. 

Riddell N, Arsenault G., Chittim B., Martin JW., McAlees A., and McCrindle R. (2009). 

Branched perfluorooctane sulfonate isomer quantification and characterization in blood 

serum samples by HPLC/ESI-MS/(/MS). Environ. Sci. Technol. 43: 7902-7908. 

WESTON. 2012. Amended Work Plan for Fish Sampling and Analysis for PFOS in 

Largemouth Bass in the Tennessee River in the Vicinity of the 3M Decatur Facility. 

Weston Solutions, Inc., West Chester, PA. 
APPENDIX A 

3M ENVIRONMENTAL LABORATORY 

ANALYTICAL DATA PACKAGES 




































APPENDIX B 

AXYS LABORATORY 

ANALYTICAL DATA PACKAGE 
2045 Mills Road West TEL 250-655-5800 FAX 250-655-5811

SIDNEY, BRITISH COLUMBIA, CANADA V8L 5X2 www.axysanalytical.com

AXYS Client No.: 4673

Client Address: Cardno ENTRIX

4295 Okemos Road, Suite 101

Okemos, MI, US, 48864

The AXYS contact for these data is Kalai Pillay.

www.axysanalytical.com Page 1 of 49
Batch ID: WG39768 Date:

Analysis Type: Matrix Type:

Tissue

Contract: 4673 Blank:

Samples: WG39768-101

L17838-1 Reference Tiss. TCR11-0039

L17838-2 MSF05D 120403

L17838-3 MSF11D 120403

L17838-4 MSF24D 120405

Reference or Spike:

WG39768-102

WG39768-104

WG39768-105

Duplicate:

WG39768-103

Comments:

1. Data are not blank corrected.

FQA-006 Rev. 2. 18-Jul-1994

Copyright AXYS Analytical Services Ltd

BATCH SUMMARY

February 1993

27-Apr-2012

BATCH MAKEUP

Perfluorinated Organic

www.axysanalytical.com Page 2 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_L17838-1_Form1A_FC2G_157S24_SJ1453688.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

Reference Tiss. TCR11-0039

Sample Collection:

N/A

Form 1A

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: L17838-1

Matrix: TISSUE Sample Size: 2.00 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 00:32:37 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 24

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

COMPOUND LAB FLAG 1 CONC.

FOUND

REPORTING

LIMIT (RL)2

RETENTION

TIME

PFOS 7.16 1.00 (L) 8:17

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-1_Form1A_FC2G_157S24_SJ1453688.html)

www.axysanalytical.com Page 3 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_L17838-1_Form2_FC2G_157S24_SJ1453688.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

Reference Tiss. TCR11-0039

Sample Collection:

N/A

Form 2

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: L17838-1

Matrix: TISSUE Sample Size: 2.00 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 00:32:37 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 24

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

LABELED COMPOUND LAB

FLAG 1

SPIKE

CONC.

CONC.

FOUND

R(%) 2 RETENTION

TIME

13C4-PFOS 36.0 31.5 87.6 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 10.6 88.5 7:04

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-1_Form2_FC2G_157S24_SJ1453688.html)

www.axysanalytical.com Page 4 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_L17838-2_Form1A_FC2G_157S28_SJ1453692.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF05D 120403

Sample Collection:

03-Apr-2012

Form 1A

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: L17838-2 (A)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:39:33 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 28

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

COMPOUND LAB FLAG 1 CONC.

FOUND

REPORTING

LIMIT (RL)2

RETENTION

TIME

PFOS 656 0.948 (L) 8:17

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-2_Form1A_FC2G_157S28_SJ1453692.html)

www.axysanalytical.com Page 5 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_L17838-2_Form2_FC2G_157S28_SJ1453692.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF05D 120403

Sample Collection:

03-Apr-2012

Form 2

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: L17838-2 (A)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:39:33 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 28

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

LABELED COMPOUND LAB

FLAG 1

SPIKE

CONC.

CONC.

FOUND

R(%) 2 RETENTION

TIME

13C4-PFOS 36.0 28.4 79.0 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 9.77 81.5 7:06

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-2_Form2_FC2G_157S28_SJ1453692.html)

www.axysanalytical.com Page 6 of 49
(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_L17838-3_Form1A_FC2G_158S8_SJ1453777.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF11D 120403

Sample Collection:

03-Apr-2012

Form 1A

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: L17838-3 N (A)

Matrix: TISSUE Sample Size: 2.15 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 16:11:38 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_158 S: 8

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: 5 Cal. Ver. Data Filename: FC2G_158 S: 4

Concentration Units: ng/g (wet weight basis)

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

COMPOUND LAB FLAG 1 CONC.

FOUND

REPORTING

LIMIT (RL)2

RETENTION

TIME

PFOS D 3720 4.65 (L) 8:21

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-3_Form1A_FC2G_158S8_SJ1453777.html)

www.axysanalytical.com Page 7 of 49
(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_L17838-3_Form2_FC2G_158S8_SJ1453777.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF11D 120403

Sample Collection:

03-Apr-2012

Form 2

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: L17838-3 N (A)

Matrix: TISSUE Sample Size: 2.15 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 16:11:38 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_158 S: 8

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: 5 Cal. Ver. Data Filename: FC2G_158 S: 4

Concentration Units: ng absolute

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

LABELED COMPOUND LAB

FLAG 1

SPIKE

CONC.

CONC.

FOUND

R(%) 2 RETENTION

TIME

13C4-PFOS D 36.0 20.4 56.5 8:21

CLEANUP STANDARD

13C8-PFOA D 12.0 8.90 74.2 7:06

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-3_Form2_FC2G_158S8_SJ1453777.html)

www.axysanalytical.com Page 8 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_L17838-4_Form1A_FC2G_157S27_SJ1453691.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF24D 120405

Sample Collection:

05-Apr-2012

Form 1A

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: L17838-4

Matrix: TISSUE Sample Size: 2.05 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:22:47 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 27

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

COMPOUND LAB FLAG 1 CONC.

FOUND

REPORTING

LIMIT (RL)2

RETENTION

TIME

PFOS 537 0.976 (L) 8:17

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-4_Form1A_FC2G_157S27_SJ1453691.html)

www.axysanalytical.com Page 9 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_L17838-4_Form2_FC2G_157S27_SJ1453691.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF24D 120405

Sample Collection:

05-Apr-2012

Form 2

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: L17838-4

Matrix: TISSUE Sample Size: 2.05 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:22:47 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 27

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

LABELED COMPOUND LAB

FLAG 1

SPIKE

CONC.

CONC.

FOUND

R(%) 2 RETENTION

TIME

13C4-PFOS 36.0 27.3 75.9 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 10.8 90.3 7:06

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-4_Form2_FC2G_157S27_SJ1453691.html)

www.axysanalytical.com Page 10 of 49
(1) Where applicable, custom lab flags have been used on this report; U = not detected at RL.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-101_Form1A_FC2G_157S22_SJ1453684.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

Lab Blank

Sample Collection:

N/A

Form 1A

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. N/A

Contract No.: 4673 Lab Sample I.D.: WG39768-101

Matrix: TISSUE Sample Size: 2.00 g

Sample Receipt Date: N/A Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 24-Apr-2012 Time: 23:59:06 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 22

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

COMPOUND LAB FLAG 1 CONC.

FOUND

REPORTING

LIMIT (RL)2

RETENTION

TIME

PFOS U 1.00 (L)

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-101_Form1A_FC2G_157S22_SJ1453684.html)

www.axysanalytical.com Page 11 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-101_Form2_FC2G_157S22_SJ1453684.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

Lab Blank

Sample Collection:

N/A

Form 2

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. N/A

Contract No.: 4673 Lab Sample I.D.: WG39768-101

Matrix: TISSUE Sample Size: 2.00 g

Sample Receipt Date: N/A Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 24-Apr-2012 Time: 23:59:06 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 22

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

LABELED COMPOUND LAB

FLAG 1

SPIKE

CONC.

CONC.

FOUND

R(%) 2 RETENTION

TIME

13C4-PFOS 36.0 33.2 92.3 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 11.2 93.7 7:04

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-101_Form2_FC2G_157S22_SJ1453684.html)

www.axysanalytical.com Page 12 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: FC-Form8A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-102_Form8A_SJ1453676.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 8A

PERFLUORINATED ORGANICS ONGOING PRECISION AND RECOVERY (OPR)

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Contract No.: 4673 Lab Sample I.D.: WG39768-102

Matrix: TISSUE Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 24-Apr-2012 Time: 22:51:55 Column ID: C18MS

Extract Volume (uL): 4000 OPR Data Filename: FC2G_157 S: 18

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

ALL CONCENTRATIONS REPORTED ON THIS FORM ARE CONCENTRATIONS IN EXTRACT, BASED ON A 1 mL EXTRACT VOLUME.

COMPOUND

LAB

FLAG 1

SPIKE CONC.

(ng/mL)

CONC.

FOUND

(ng/mL) % RECOVERY

RETENTION

TIME

PFOS 80.0 87.1 109 8:17

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-102_Form8A_SJ1453676.html)

www.axysanalytical.com Page 13 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: FC-Form8B.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-102_Form8B_SJ1453676.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 8B

PERFLUORINATED ORGANICS ONGOING PRECISION AND RECOVERY (OPR)

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Contract No.: 4673 Lab Sample I.D.: WG39768-102

Matrix: TISSUE Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 24-Apr-2012 Time: 22:51:55 Column ID: C18MS

Extract Volume (uL): 4000 OPR Data Filename: FC2G_157 S: 18

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

ALL CONCENTRATIONS REPORTED ON THIS FORM ARE CONCENTRATIONS IN EXTRACT, BASED ON A 1 mL EXTRACT VOLUME.

LABELED

COMPOUND

LAB

FLAG 1

SPIKE CONC.

(ng/mL)

CONC.

FOUND

(ng/mL) % RECOVERY

RETENTION

TIME

13C4-PFOS 36.0 29.0 80.5 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 11.2 93.3 7:04

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-102_Form8B_SJ1453676.html)

www.axysanalytical.com Page 14 of 49
(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-103_Form1A_FC2G_158S9_SJ1453778.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF11D 120403 (Duplicate)

Sample Collection:

03-Apr-2012

Form 1A

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: WG39768-103 N (DUP L17838-3)

Matrix: TISSUE Sample Size: 2.07 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 16:28:24 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_158 S: 9

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: 5 Cal. Ver. Data Filename: FC2G_158 S: 4

Concentration Units: ng/g (wet weight basis)

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

COMPOUND LAB FLAG 1 CONC.

FOUND

REPORTING

LIMIT (RL)2

RETENTION

TIME

PFOS D 3510 4.83 (L) 8:21

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-103_Form1A_FC2G_158S9_SJ1453778.html)

www.axysanalytical.com Page 15 of 49
(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-103_Form2_FC2G_158S9_SJ1453778.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF11D 120403 (Duplicate)

Sample Collection:

03-Apr-2012

Form 2

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: WG39768-103 N (DUP L17838-3)

Matrix: TISSUE Sample Size: 2.07 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 16:28:24 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_158 S: 9

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: 5 Cal. Ver. Data Filename: FC2G_158 S: 4

Concentration Units: ng absolute

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

LABELED COMPOUND LAB

FLAG 1

SPIKE

CONC.

CONC.

FOUND

R(%) 2 RETENTION

TIME

13C4-PFOS D 36.0 25.9 72.0 8:21

CLEANUP STANDARD

13C8-PFOA D 12.0 10.7 89.2 7:06

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-103_Form2_FC2G_158S9_SJ1453778.html)

www.axysanalytical.com Page 16 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-104_Form1A_FC2G_157S29_SJ1453693.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF05D 120403 (MS)

Sample Collection:

03-Apr-2012

Form 1A

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: WG39768-104 (MS)

Matrix: TISSUE Sample Size: 2.01 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:56:19 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 29

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

COMPOUND LAB FLAG 1 CONC.

FOUND

REPORTING

LIMIT (RL)2

RETENTION

TIME

PFOS 670 0.995 (L) 8:17

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-104_Form1A_FC2G_157S29_SJ1453693.html)

www.axysanalytical.com Page 17 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-104_Form2_FC2G_157S29_SJ1453693.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF05D 120403 (MS)

Sample Collection:

03-Apr-2012

Form 2

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: WG39768-104 (MS)

Matrix: TISSUE Sample Size: 2.01 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:56:19 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 29

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

LABELED COMPOUND LAB

FLAG 1

SPIKE

CONC.

CONC.

FOUND

R(%) 2 RETENTION

TIME

13C4-PFOS 36.0 35.4 98.2 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 11.0 91.3 7:06

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-104_Form2_FC2G_157S29_SJ1453693.html)

www.axysanalytical.com Page 18 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-105_Form1A_FC2G_157S30_SJ1453694.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF05D 120403 (MSD)

Sample Collection:

03-Apr-2012

Form 1A

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: WG39768-105 (MSD)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 02:13:05 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 30

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

COMPOUND LAB FLAG 1 CONC.

FOUND

REPORTING

LIMIT (RL)2

RETENTION

TIME

PFOS 653 0.948 (L) 8:17

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-105_Form1A_FC2G_157S30_SJ1453694.html)

www.axysanalytical.com Page 19 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFC_FC_LC_PFOA_WG39768-105_Form2_FC2G_157S30_SJ1453694.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF05D 120403 (MSD)

Sample Collection:

03-Apr-2012

Form 2

PERFLUORINATED ORGANICS ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: WG39768-105 (MSD)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 02:13:05 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 30

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute

This page is part of a total report that contains information necessary for accreditation compliance.

Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.

LABELED COMPOUND LAB

FLAG 1

SPIKE

CONC.

CONC.

FOUND

R(%) 2 RETENTION

TIME

13C4-PFOS 36.0 37.1 103 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 10.9 91.1 7:04

Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-105_Form2_FC2G_157S30_SJ1453694.html)

www.axysanalytical.com Page 20 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Kristina Coleman___________

For Axys Internal Use Only [ XSL Template: FC-Form3A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFOA_FC_LC_24-Apr-2012_FC2G__Form3A_GS45507.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 3A

PERFLUORINATED ORGANICS INITIAL CALIBRATION PERCENT RECOVERIES

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

CS0 Data Filename: FC2G_157 S: 4

Initial Calibration Date: 24-Apr-2012 CS1 Data Filename: FC2G_157 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_157 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_157 S: 7

CS4 Data Filename: FC2G_157 S: 8

CS5 Data Filename: FC2G_157 S: 9

CS6 Data Filename: FC2G_157 S: 10

CS7 Data Filename: FC2G_157 S: 11

CS8 Data Filename: N/A

PERCENT RECOVERY (%)

CS0 CS1 CS2 CS3 CS4 CS5 CS6 CS7 CS8

COMPOUND LAB

FLAG 1

PFOS 104 91.9 86.4 105 99.5 112 101 99.7

Page 1 of 1 (WG39768 - PFOA_FC_LC_24-Apr-2012_FC2G__Form3A_GS45507.html)

www.axysanalytical.com Page 21 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Kristina Coleman___________

For Axys Internal Use Only [ XSL Template: FC-Form3B.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFOA_FC_LC_24-Apr-2012_FC2G__Form3B_GS45507.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 3B

PERFLUORINATED ORGANICS INITIAL CALIBRATION PERCENT RECOVERIES

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

CS0 Data Filename: FC2G_157 S: 4

Initial Calibration Date: 24-Apr-2012 CS1 Data Filename: FC2G_157 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_157 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_157 S: 7

CS4 Data Filename: FC2G_157 S: 8

CS5 Data Filename: FC2G_157 S: 9

CS6 Data Filename: FC2G_157 S: 10

CS7 Data Filename: FC2G_157 S: 11

CS8 Data Filename: N/A

PERCENT RECOVERIES (%)

CS0 CS1 CS2 CS3 CS4 CS5 CS6 CS7 CS8

LABELED COMPOUND LAB

FLAG 1

13C4-PFOS 103 82.4 92.7 86.9 104 103 111 117

CLEAN-UP STANDARD

13C8-PFOA 101 99.6 94.3 98.3 101 98.9 103 104

Page 1 of 1 (WG39768 - PFOA_FC_LC_24-Apr-2012_FC2G__Form3B_GS45507.html)

www.axysanalytical.com Page 22 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Kristina Coleman___________

For Axys Internal Use Only [ XSL Template: FC-Form3C.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFOA_FC_LC_24-Apr-2012_FC2G__Form3C_GS45507.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 3C

PERFLUORINATED ORGANICS INITIAL CALIBRATION RETENTION TIMES

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

CS0 Data Filename: FC2G_157 S: 4

Initial Calibration Date: 24-Apr-2012 CS1 Data Filename: FC2G_157 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_157 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_157 S: 7

CS4 Data Filename: FC2G_157 S: 8

CS5 Data Filename: FC2G_157 S: 9

CS6 Data Filename: FC2G_157 S: 10

CS7 Data Filename: FC2G_157 S: 11

CS8 Data Filename: N/A

RETENTION TIMES

CS0 CS1 CS2 CS3 CS4 CS5 CS6 CS7 CS8 MEAN

RT

COMPOUND LAB

FLAG 1

PFOS 8:17 8:17 8:17 8:17 8:17 8:17 8:17 8:17 8:17

Page 1 of 1 (WG39768 - PFOA_FC_LC_24-Apr-2012_FC2G__Form3C_GS45507.html)

www.axysanalytical.com Page 23 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Kristina Coleman___________

For Axys Internal Use Only [ XSL Template: FC-Form3D.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFOA_FC_LC_24-Apr-2012_FC2G__Form3D_GS45507.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 3D

PERFLUORINATED ORGANICS INITIAL CALIBRATION RETENTION TIMES

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

CS0 Data Filename: FC2G_157 S: 4

Initial Calibration Date: 24-Apr-2012 CS1 Data Filename: FC2G_157 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_157 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_157 S: 7

CS4 Data Filename: FC2G_157 S: 8

CS5 Data Filename: FC2G_157 S: 9

CS6 Data Filename: FC2G_157 S: 10

CS7 Data Filename: FC2G_157 S: 11

CS8 Data Filename: N/A

RETENTION TIMES

CS0 CS1 CS2 CS3 CS4 CS5 CS6 CS7 CS8 MEAN

RT

LABELED COMPOUND LAB

FLAG1

13C4-PFOS 8:17 8:17 8:17 8:17 8:21 8:17 8:17 8:17 8:18

CLEAN-UP STANDARD

13C8-PFOA 7:04 7:04 7:04 7:04 7:04 7:04 7:04 7:04 7:04

Page 1 of 1 (WG39768 - PFOA_FC_LC_24-Apr-2012_FC2G__Form3D_GS45507.html)

www.axysanalytical.com Page 24 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form4A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFOA_FC_LC_FC2G_157S15__Form4A_SJ1453671.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 4A

PERFLUORINATED ORGANICS CALIBRATION VERIFICATION

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Initial Calibration Date: 24-Apr-2012 VER Data Filename: FC2G_157 S: 15

Instrument ID: LC MS/MS Analysis Date: 24-Apr-2012

LC Column ID: C18MS Analysis Time: 22:01:37

COMPOUND LAB

FLAG 1

RETENTION TIME EXPECTED CONC.

(ng)

CONC. FOUND

(ng)

RECOVERY (%)

PFOS 8:17 80.0 86.8 108

Page 1 of 1 (WG39768 - PFOA_FC_LC_FC2G_157S15__Form4A_SJ1453671.html)

www.axysanalytical.com Page 25 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form4B.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFOA_FC_LC_FC2G_157S15__Form4B_SJ1453671.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 4B

PERFLUORINATED ORGANICS CALIBRATION VERIFICATION

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Initial Calibration Date: 24-Apr-2012 VER Data Filename: FC2G_157 S: 15

Instrument ID: LC MS/MS Analysis Date: 24-Apr-2012

LC Column ID: C18MS Analysis Time: 22:01:37

LABELED COMPOUND LAB

FLAG 1

RETENTION TIME EXPECTED CONC.

(ng)

CONC. FOUND

(ng)

RECOVERY (%)

13C4-PFOS 8:17 36.0 36.0 100

CLEANUP STANDARD

13C8-PFOA 7:06 12.0 12.1 101

Page 1 of 1 (WG39768 - PFOA_FC_LC_FC2G_157S15__Form4B_SJ1453671.html)

www.axysanalytical.com Page 26 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form4A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFOA_FC_LC_FC2G_158S4__Form4A_SJ1453773.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 4A

PERFLUORINATED ORGANICS CALIBRATION VERIFICATION

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Initial Calibration Date: 24-Apr-2012 VER Data Filename: FC2G_158 S: 4

Instrument ID: LC MS/MS Analysis Date: 25-Apr-2012

LC Column ID: C18MS Analysis Time: 15:04:34

COMPOUND LAB

FLAG 1

RETENTION TIME EXPECTED CONC.

(ng)

CONC. FOUND

(ng)

RECOVERY (%)

PFOS 8:17 80.0 81.1 101

Page 1 of 1 (WG39768 - PFOA_FC_LC_FC2G_158S4__Form4A_SJ1453773.html)

www.axysanalytical.com Page 27 of 49
(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

For Axys Internal Use Only [ XSL Template: FC-Form4B.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13;

Report Filename: PFOA_FC_LC_FC2G_158S4__Form4B_SJ1453773.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

Form 4B

PERFLUORINATED ORGANICS CALIBRATION VERIFICATION

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Initial Calibration Date: 24-Apr-2012 VER Data Filename: FC2G_158 S: 4

Instrument ID: LC MS/MS Analysis Date: 25-Apr-2012

LC Column ID: C18MS Analysis Time: 15:04:34

LABELED COMPOUND LAB

FLAG 1

RETENTION TIME EXPECTED CONC.

(ng)

CONC. FOUND

(ng)

RECOVERY (%)

13C4-PFOS 8:21 36.0 28.3 78.6

CLEANUP STANDARD

13C8-PFOA 7:06 12.0 11.8 98.3

Page 1 of 1 (WG39768 - PFOA_FC_LC_FC2G_158S4__Form4B_SJ1453773.html)

www.axysanalytical.com Page 28 of 49
(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: RPD.xsl; Created: 27-Apr-2012 15:00:24; Application: XMLTransformer-1.12.13;

Report Filename: RPD_FC_LC_PFOA-RPD_WG39768-103_L17838-3_.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8

PERFLUORINATED ORGANICS ANALYSIS REPORT

RELATIVE PERCENT DIFFERENCE

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673

Client ID: MSF11D 120403 Concentration Units: ng/g (wet weight basis)

L17838-3 (A) WG39768-103

COMPOUND LAB

FLAG 1

CONC.

FOUND

LAB

FLAG 1

CONC.

FOUND

MEAN RELATIVE

PERCENT

DIFFERENCE

PFOS D 3720 D 3510 3620 5.77

Page 1 of 1 (WG39768 - RPD_FC_LC_PFOA-RPD_WG39768-103_L17838-3_.html)

www.axysanalytical.com Page 29 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) R% = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: MS.xsl; Created: 27-Apr-2012 15:00:16; Application: XMLTransformer-1.12.13;

Report Filename: MS_FC_LC_PFOA-MS-MSD_WG39768-104_L17838-2_Form8C.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF05D 120403 (MS)

Sample Collection:

03-Apr-2012

Form 8C

PERFLUORINATED ORGANICS MATRIX SPIKE (MS)

ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: WG39768-104 (MS)

Matrix: TISSUE Sample Size: 2.01 g (wet)

Extraction Date: 23-Apr-2012 Initial Calibration Date: 24-Apr-2012

Analysis Date: 25-Apr-2012 Time: 01:56:19 Instrument ID: LC MS/MS

Extract Volume (uL): 4000 Column ID: C18MS

Injection Volume (uL): 15 MS Data Filename: FC2G_157 S: 29

Dilution Factor: N/A Blank Data Filename: FC2G_157 S: 22

Cal. Ver. Data Filename: FC2G_157 S: 15

ALL CONCENTRATIONS REPORTED ON THIS FORM ARE CONCENTRATIONS ON SAMPLE SIZE BASIS

COMPOUND LAB

FLAG 1

ION

ABUND.

RATIO

SPIKE

CONC

(ng/g)

SAMPLE

LAB

FLAG 1

SAMPLE

CONC

(ng/g)

CONC.

FOUND

(ng/g)

MS

R% 2

REL

%

DIFF

PFOS N/A 39.8 656 670 36.4

Page 1 of 1 (WG39768 - MS_FC_LC_PFOA-MS-MSD_WG39768-104_L17838-2_Form8C.html)

www.axysanalytical.com Page 30 of 49
(1) Where applicable, custom lab flags have been used on this report.

(2) R% = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes.

Signed: ___________Bryan Alonzo___________

These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: MS.xsl; Created: 27-Apr-2012 15:00:16; Application: XMLTransformer-1.12.13;

Report Filename: MS_FC_LC_PFOA-MS-MSD_WG39768-105_L17838-2_Form8E.html; Workgroup: WG39768; Design ID: 1722 ]

AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO.

MSF05D 120403 (MSD)

Sample Collection:

03-Apr-2012

Form 8E

PERFLUORINATED ORGANICS MATRIX SPIKE DUPLICATE (MSD)

ANALYSIS REPORT

AXYS ANALYTICAL SERVICES

2045 MILLS RD., SIDNEY, B.C., CANADA

V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Project No. 3M - ALABAMA

Contract No.: 4673 Lab Sample I.D.: WG39768-105 (MSD)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Extraction Date: 23-Apr-2012 Initial Calibration Date: 24-Apr-2012

Analysis Date: 25-Apr-2012 Time: 02:13:05 Instrument ID: LC MS/MS

Extract Volume (uL): 4000 Column ID: C18MS

Injection Volume (uL): 15 MSD Data Filename: FC2G_157 S: 30

Dilution Factor: N/A Blank Data Filename: FC2G_157 S: 22

Cal. Ver. Data Filename: FC2G_157 S: 15

ALL CONCENTRATIONS REPORTED ON THIS FORM ARE CONCENTRATIONS ON SAMPLE SIZE BASIS

COMPOUND LAB

FLAG 1

ION

ABUND.

RATIO

SPIKE

CONC

(ng/g)

SAMPLE

LAB

FLAG 1

SAMPLE

CONC

(ng/g)

CONC.

FOUND

(ng/g)

MSD

R% 2

REL

%

DIFF

PFOS N/A 37.9 656 653

Page 1 of 1 (WG39768 - MS_FC_LC_PFOA-MS-MSD_WG39768-105_L17838-2_Form8E.html)

www.axysanalytical.com Page 31 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 

Table 1a 

NELAP Accreditation Held by AXYS Analytical Services Ltd. 

 for Chlorinated Dioxins/Furans, Chlorinated Pesticides, PCBs and PAHs

Matrix Codes for Table 1a NPW = Non-Potable Water DrW = Drinking WaterS = Solid T = Tissue Accreditation Method Codes and Explanation for Table 1 Code Accreditation Certificate Applicable AXYS Method and Description

No. Method Reference

1 EPA 1613B MLA-017, performance based implementation of EPA1613B (GC/HRMS) 

2 EPA 8290 MLA-017, performance based implementation of EPA 8290 (GC/HRMS) 3 AXYS MLA-017 MLA-017, performance based implementation of EPA 1613B, 8290 (GC/HRMS) 

4 EPA 608 MLA-007, performance based implementation of EPA 608 (GC/ECD) 

5 EPA 8270C or 8270D MLA-007, performance based modification of 8270C/D (GC/LRMS) 

6 EPA 8081A or 8081B MLA-007, performance based implementation of EPA 8081A/B (GC/ECD) 7 EPA 1668A MLA-010, performance based implementation of EPA 1668A (GC/HRMS) 8 SM 6630B MLA-007, performance based implementation of SM 18-20 6630B (GC/ECD) 9 EPA 1625B MLA-021, performance based modification of EPA 1625B (GC/LRMS) 

11 EPA 625 MLA-007, performance based modification of EPA 625 (GC/LRMS) 

20 EPA 8270C or 8270D MLA-021, performance based modification of EPA 8270C/D (GC/LRMS) 

New York 

State 

Department 

of Health 

California 

Department 

of Public 

Health 

State of Florida 

Department 

of Health 

State of New 

Departm

Environm

Protec

Lab ID 

11674 

NELAP 

Primary 

Lab ID 

01138CA 

NELAP 

Secondary 

Lab ID E871007 

NELAP Primary 

Lab ID CA

NELAP Se

TABLE 1 

NP

W S NPW S Dr. W NP W S T Dr. W NP W 

PCDD/F - Polychlorinated Dioxins and Furans Dioxins 1 Dioxins and Dibenzofurans 2 1,2,3,4,6,7,8-HpCDD 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,4,6,7,8-HpCDF 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,4,7,8,9-HpCDF 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,4,7,8-HxCDD 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,4,7,8-HxCDF 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,6,7,8-HxCDD 1 2 1, 2, 3 2, 3 2, 3 1 

www.axysanalytical.com
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 

New York 

State 

Department 

of Health 

California 

Department 

of Public 

Health 

State of Florida 

Department 

of Health 

State of New 

Departm

Environm

Protec

Lab ID 

11674 

NELAP 

Primary 

Lab ID 

01138CA 

NELAP 

Secondary 

Lab ID E871007 

NELAP Primary 

Lab ID CA

NELAP Se

TABLE 1 

NP

W S NPW S Dr. W NP W S T Dr. W NP W 

1,2,3,6,7,8-HxCDF 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,7,8,9-HxCDD 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,7,8,9-HxCDF 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,7,8-PeCDD 1 2 1, 2, 3 2, 3 2, 3 1 1,2,3,7,8-PeCDF 1 2 1, 2, 3 2, 3 2, 3 1 2,3,4,6,7,8-HxCDF 1 2 1, 2, 3 2, 3 2, 3 1 2,3,4,7,8-PeCDF 1 2 1, 2, 3 2, 3 2, 3 1 2,3,7,8-TCDD 1 1 2 1, 2, 3 2, 3 2, 3 1 2,3,7,8-TCDF 1 2 1, 2, 3 2, 3 2, 3 1 OCDD 1 2 1, 2, 3 2, 3 2, 3 1 OCDF 1 2 1, 2, 3 2, 3 2, 3 1 Total TCDD 1 1, 2, 3 2, 3 2, 3 Total TCDF 1 1, 2, 3 2, 3 2, 3 Total PeCDD 1 1, 2, 3 2, 3 2, 3 Total PeCDF 1 1, 2, 3 2, 3 2, 3 Total HxCDD 1 1, 2, 3 2, 3 2, 3 Total HxCDF 1 1, 2, 3 2, 3 2, 3 Total HpCDD 1 1, 2, 3 2, 3 2, 3 Total HpCDF 1 1, 2, 3 2, 3 2, 3 PCBs – Polychlorinated biphenyls PCB 1 2-Chlorobiphenyl 7 7 7 PCB 3 4-Chlorobiphenyl 7 7 7 PCB 4 2,2'-Dichlorobiphenyl 7 7 7 PCB 5 2,3-Dichlorobiphenyl 7 7 7 PCB 15 4,4'-Dichlorobiphenyl 7 7 7 PCB 18 2,2',5-Trichlorobiphenyl 7 7 7 PCB 19 2,2',6-Trichlorobiphenyl 7 7 7 PCB 31 2,4',5-Trichlorobiphenyl 7 7 7 PCB 37 3,4,4'-Trichlorobiphenyl 7 7 7 PCB 44 2,2',3,5'-Tetrachlorobiphenyl 7 7 7 PCB 52 2,2',5,5'-Tetrachlorobiphenyl 7 7 7 PCB 54 2,2',6,6'-Tetrachlorobiphenyl 7 7 7 PCB 66 2,3',4,4'-Tetrachlorobiphenyl 7 7 7 PCB 77 3,3',4,4'-Tetrachlorobiphenyl 7 7 7 PCB 81 3,4,4',5-Tetrachlorobiphenyl 7 7 7 PCB 87 2,2',3,4,5'-Pentachlorobiphenyl 7 7 7 

www.axysanalytical.com
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 

New York 

State 

Department 

of Health 

California 

Department 

of Public 

Health 

State of Florida 

Department 

of Health 

State of New 

Departm

Environm

Protec

Lab ID 

11674 

NELAP 

Primary 

Lab ID 

01138CA 

NELAP 

Secondary 

Lab ID E871007 

NELAP Primary 

Lab ID CA

NELAP Se

TABLE 1 

NP

W S NPW S Dr. W NP W S T Dr. W NP W 

PCB 101 2,2',4,5,5'-Pentachlorobiphenyl 7 7 7 PCB 104 2,2',4,6,6'-Pentachlorobiphenyl 7 7 7 PCB 105 2,3,3',4,4'-Pentachlorobiphenyl 7 7 7 PCB 109 2,3,3',4,6-Pentachlorobiphenyl 7 7 7 PCB 114 2,3,4,4',5-Pentachlorobiphenyl 7 7 7 PCB 118 2,3',4,4',5-Pentachlorobiphenyl 7 7 7 PCB 123 2,3',4,4',5'-Pentachlorobiphenyl 7 7 7 PCB 124 2,3',4',5,5'-Pentachlorobiphenyl 7 PCB 126 3,3',4,4',5-Pentachlorobiphenyl 7 7 7 PCB 138 2,2',3,4,4',5'-Hexachlorobiphenyl 7 7 7 PCB 141 2,2',3,4,5,5'-Hexachlorobiphenyl 7 7 7 PCB 151 2,2',3,5,5',6-Hexachlorobiphenyl 7 7 7 PCB 153 2,2',4,4',5,5'-Hexachlorobiphenyl 7 7 7 PCB 155 2,2',4,4',6,6'-Hexachlorobiphenyl 7 7 7 PCB 156 2,3,3',4,4',5-Hexachlorobiphenyl 7 7 PCB 157 2,3,3',4,4',5'-Hexachlorobiphenyl 7 7 7 PCB 167 2,3',4,4',5,5'-Hexachlorobiphenyl 7 7 7 PCB 169 3,3',4,4',5,5'-Hexachlorobiphenyl 7 7 7 PCB 170 2,2',3,3',4,4',5-Heptachlorobiphenyl 7 7 7 PCB 180 2,2',3,4,4',5,5'-Heptachlorobiphenyl 7 7 7 PCB 183 2,2',3,4,4',5',6-Heptachlorobiphenyl 7 7 7 PCB 187 2,2',3,4',5,5',6-Heptachlorobiphenyl 7 7 7 PCB 188 2,2',3,4',5,6,6'-Heptachlorobiphenyl 7 7 7 PCB 189 2,3,3',4,4',5,5'-Heptachlorobiphenyl 7 7 7 PCB 202 2,2',3,3',5,5',6,6'-Octachlorobiphenyl 7 7 7 PCB 205 2,3,3',4,4',5,5',6-Octachlorobiphenyl 7 7 7 PCB 206 2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl 7 7 7 PCB 208 2,2',3,3',4,5,5',6,6'-Nonachlorobiphenyl 7 7 7 PCB 209 Decachlorobiphenyl 7 7 7 Aroclor 1260 7, 11 5, 7 11 5 Aroclor 1254 7, 11 5, 7 11 5 Aroclor 1221 7, 11 5, 7 11 5 Aroclor 1232 7, 11 5, 7 11 5 Aroclor 1248 7, 11 5, 7 11 5 Aroclor 1016 7, 11 5, 7 11 5 Aroclor 1242 7, 11 5, 7 11 5 

www.axysanalytical.com
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 

New York 

State 

Department 

of Health 

California 

Department 

of Public 

Health 

State of Florida 

Department 

of Health 

State of New 

Departm

Environm

Protec

Lab ID 

11674 

NELAP 

Primary 

Lab ID 

01138CA 

NELAP 

Secondary 

Lab ID E871007 

NELAP Primary 

Lab ID CA

NELAP Se

TABLE 1 

NP

W S NPW S Dr. W NP W S T Dr. W NP W 

Pesticides 4,4'-DDD 11 5 11 5 4,4'-DDE 11 5 11 5 4,4'-DDT 11 5 11 5 Aldrin 11 5 11 5 Alpha-HCH 11 5 11 5 Beta-HCH 11 5 11 5 cis-Chlordane (alpha-Chlordane) 5 5 Chlordane, technical 5, 11 5 11 5 Delta-HCH 11 5 11 5 Dieldrin 4 6 4 6 Endosulphan I 4 6 4 6 Endosulphan II 4 6 4 6 Endosulphan sulphate 4 6 4 6 Endrin 4 6 4 6 Endrin aldehyde 4 6 4 6 trans-Chlordane (gamma-Chlordane) 5 5 Gamma-HCH (Lindane) 11 5 11 5 Heptachlor 11 5 11 5 Heptachlor epoxide 4 6 4 6 Hexachlorobenzene 9 5 9 5 Methoxychlor 4,8 6 8 6 Mirex 5 PAH Anthracene 9 20 9 20Pyrene 9 20 9 20Benzo[ghi]perylene 9 20 9 20Indeno[1,2,3-cd]pyrene 9 20 9 20Benzo[b]fluoranthene 9 20 9 20Fluoranthene 9 20 9 20Benzo[k]fluoranthene 9 20 9 20Acenaphthylene 9 20 9 20Chrysene 9 20 9 20Benzo[a]pyrene 9 20 9 20Dibenz[ah]anthracene 9 20 9 20Benz[a]anthracene 9 20 9 20

www.axysanalytical.com
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 

New York 

State 

Department 

of Health 

California 

Department 

of Public 

Health 

State of Florida 

Department 

of Health 

State of New 

Departm

Environm

Protec

Lab ID 

11674 

NELAP 

Primary 

Lab ID 

01138CA 

NELAP 

Secondary 

Lab ID E871007 

NELAP Primary 

Lab ID CA

NELAP Se

TABLE 1 

NP

W S NPW S Dr. W NP W S T Dr. W NP W 

Acenaphthene 9 20 9 20Phenanthrene 9 20 9 20Fluorene 9 20 9 20Naphthalene 9 20 9 20

www.axysanalytical.com
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 

Table 1b 

NELAP Accreditation Held by AXYS Analytical Services Ltd. 

for Perfluorinated Organic Compounds

Matrix Codes for Table 1b NPW = Non-Potable Water DrW = Drinking WaterS = Solid T = Tissue Accreditation Method Codes and Explanation for Table 1b Code Accreditation Certificate Applicable AXYS Method and Description

No. Method Reference

12 AXYS MLA-041 MLA-041, laboratory performance based method (LC/MS-MS) 13 AXYS MLA-043 MLA-043, laboratory performance based method (LC/MS-MS) 14 AXYS MLA-060 MLA-060, laboratory performance based method (LC/MS-MS) 

State of Florida 

Department 

of Health

Minnesota Department 

of Health

State of New 

Departm

Environm

Protec

Lab ID E871007 

NELAP Primary

Lab ID 232-999-430 

NELAP Primary

Lab ID CA

NELAP Se

TABLE 1 

 Dr. 

W

NP 

W S T Dr. W NP W S T Dr. W NP W 

PFC – Perfluorinated Organic Compounds Perfluorobutanoate (PFBA) Note 14 14 12 13 14 14 12 13 14 14 Perfluoropentanoate (PFPeA) Note 14 14 12 13 14 14 12 13 14 14 Perfluorohexanoate (PFHxA) Note 14 14 12 13 14 14 12 13 14 14 Perfluoroheptanoate (PFHpA) Note 14 14 12 13 14 14 12 13 14 14 Perfluorooctanoate (PFOA) Note 14 14 12 13 14 14 12 13 14 14 Perfluorononanoate (PFNA) Note 14 14 12 13 14 14 12 13 14 14 Perfluorodecanoate (PFDA) Note 14 14 12 13 14 14 12 13 14 14 Perfluoroundecanoate (PFUnA) Note 14 14 12 13 14 14 12 13 14 14 Perfluorododecanoate (PFDoA) Note 14 14 12 13 14 14 12 13 14 14 Perfluorobutanesulfonate (PFBS) 14 14 12 13 14 14 12 13 14 14 Perfluorohexanesulfonate (PFHxS) 14 14 12 13 14 14 12 13 14 14 Perfluorooctanesulfonate (PFOS) 14 14 12 13 14 14 12 13 14 14 Perfluorooctane sulfonamide (PFOSA) 14 14 12 13 14 14 12 13 Note: Accreditations by Minnesota Department of Health and New Jersey Department of Environmental Protection are against the corresponding 

www.axysanalytical.com
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 7 of 18 

Table 2: 

Canadian and US State Specific Accreditation Held by AXYS Analytical Services Ltd. 

Matrix Codes for Table 2 

NP W = Non-Potable Water 

Dr. W = Drinking Water 

W = Aqueous 

S = Solid 

T = Tissue 

Accreditation Method Codes and Explanation for Table 2 

Code Accreditation Certificate Applicable AXYS Method and Description

No. Method Reference

1 EPA 1613 MLA-017 Performance based implementation of EPA 1613B (GC/HRMS) 

3 AXYS MLA-017 MLA-017 Performance based implementation of EPA 1613B (GC/HRMS) 

7 EPA 1668A MLA-010 Performance based implementation of EPA 1668A (GC/HRMS) 

10 AXYS MLA-007 MLA-007, Performance based modification of EPA 8270C/D, 8081A/B 

 (GC/LRMS and GC/ECD) 

12 AXYS MLA-041 MLA-041 Laboratory performance based method (LC/MS-MS) 

13 AXYS MLA-043 MLA-043 Laboratory performance based method (LC/MS-MS) 

14 AXYS MLA-060 MLA-060 Laboratory performance based method (LC/MS-MS) 

15 AXYS MLA-010 MLA-010 Performance based implementation of EPA 1668A (GC/HRMS) 

16 AXYS MLA-028 MLA-028 Laboratory performance based method (GC/HRMS) 

17 AXYS MLA-033 MLA-033 Performance based implementation of EPA 1614 (GC/HRMS) 

18 AXYS MLA-021 MLA-021 Performance based modification of EPA 8270C/D (GC/LRMS) 

19 AXYS MLA-075 MLA-075 Performance based implementation of EPA 1694 (LC/MS-MS) 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

PCDD/F - Polychlorinated Dioxins and Furans 

1,2,3,4,6,7,8-HpCDD 3 3 3 3 1 1 

1,2,3,4,6,7,8-HpCDF 3 3 3 3 1 1 

1,2,3,4,7,8,9-HpCDF 3 3 3 3 1 1 

1,2,3,4,7,8-HxCDD 3 3 3 3 1 1 

1,2,3,4,7,8-HxCDF 3 3 3 3 1 1 

1,2,3,6,7,8-HxCDD 3 3 3 3 1 1 

1,2,3,6,7,8-HxCDF 3 3 3 3 1 1 

1,2,3,7,8,9-HxCDD 3 3 3 3 1 1 

1,2,3,7,8,9-HxCDF 3 3 3 3 1 1 

1,2,3,7,8-PeCDD 3 3 3 3 1 1 

1,2,3,7,8-PeCDF 3 3 3 3 1 1 

2,3,4,6,7,8-HxCDF 3 3 3 3 1 1 

2,3,4,7,8-PeCDF 3 3 3 3 1 1 

2,3,7,8-TCDD 3 3 3 3 1 1 

2,3,7,8-TCDF 3 3 3 3 1 1 

OCDD 3 3 3 3 1 1 

OCDF 3 3 3 3 1 1 

Total TCDD 1 1 

Total TCDF 1 1 

Total PeCDD 1 1 

Total PeCDF 1 1 

Total HxCDD 1 1 

www.axysanalytical.com Page 38 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 8 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

Total HxCDF 1 1 

Total HpCDD 1 1 

Total HpCDF 1 1 

Total PCDD 1 1 

Total PCDF 1 1 

Total PCDD + PCDF 1 1 

 

PCBs – Polychlorinated biphenyls 

PCB 1 2-Chlorobiphenyl 15 15 15 7 7 

PCB 2 3-Chlorobiphenyl 15 15 15 7 7 

PCB 3 4-Chlorobiphenyl 15 15 15 7 7 

PCB 4 2,2'-Dichlorobiphenyl 15 15 15 7 7 

PCB 5 2,3-Dichlorobiphenyl 15 15 15 7 7 

PCB 6 2,3'-Dichlorobiphenyl 15 15 15 7 7 

PCB 7 2,4-Dichlorobiphenyl 15 15 15 7 7 

PCB 8 2,4'-Dichlorobiphenyl 15 15 15 7 7 

PCB 8/5 10 10 10 

PCB 9 2,5-Dichlorobiphenyl 15 15 15 7 7 

PCB 10 2,6-Dichlorobiphenyl 15 15 15 7 7 

PCB 11 3,3'-Dichlorobiphenyl 15 15 15 7 7 

PCB 12 3,4-Dichlorobiphenyl 15 15 15 7 7 

PCB 13 3,4'-Dichlorobiphenyl 15 15 15 7 7 

PCB 14 3,5-Dichlorobiphenyl 15 15 15 7 7 

PCB 15 4,4'-Dichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 16 2,2',3-Trichlorobiphenyl 15 15 15 7 7 

PCB 16/32 10 10 10 

PCB 17 2,2',4-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 18 2,2',5-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 19 2,2',6-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 20 2,3,3'-Trichlorobiphenyl 15 15 15 7 7 

PCB 21 2,3,4-Trichlorobiphenyl 15 15 15 7 7 

PCB 22 2,3,4'-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 23 2,3,5-Trichlorobiphenyl 15 15 15 7 7 

PCB 24 2,3,6-Trichlorobiphenyl 15 15 15 7 7 

PCB 24/27 10 10 10 

PCB 25 2,3',4-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 26 2,3',5-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 27 2,3',6-Trichlorobiphenyl 15 15 15 7 7 

PCB 28 2,4,4'-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 29 2,4,5-Trichlorobiphenyl 15 15 15 7 7 

PCB 30 2,4,6-Trichlorobiphenyl 15 15 15 7 7 

PCB 31 2,4',5-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 32 2,4',6-Trichlorobiphenyl 15 15 15 7 7 

PCB 33 2,3',4'-Trichlorobiphenyl 15 15 15 7 7 

PCB 33/20/21 18 10 10 

PCB 34 2,3',5'-Trichlorobiphenyl 15 15 15 7 7 

PCB 35 3,3',4-Trichlorobiphenyl 15 15 15 7 7 

PCB 36 3,3',5-Trichlorobiphenyl 15 15 15 7 7 

PCB 37 3,4,4'-Trichlorobiphenyl 15 15 15 7 7 

PCB 38 3,4,5-Trichlorobiphenyl 15 15 15 7 7 

PCB 39 3,4',5-Trichlorobiphenyl 15 15 15 7 7 

PCB 40 2,2',3,3'-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 41 2,2',3,4-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 41/71/64/68 10 10 10 

www.axysanalytical.com Page 39 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 9 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

PCB 42 2,2',3,4'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 42/59 10 10 10 

PCB 43 2,2',3,5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 44 2,2',3,5'-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 45 2,2',3,6-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 46 2,2',3,6'-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 47 2,2',4,4'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 47/48/75 10 10 10 

PCB 48 2,2',4,5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 49 2,2',4,5'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 49/43 10 10 10 

PCB 50 2,2',4,6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 51 2,2',4,6'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 52 2,2',5,5'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 52/73 10 10 10 

PCB 53 2,2',5,6'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 54 2,2',6,6'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 55 2,3,3',4-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 56 2,3,3',4'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 56/60 10 10 10 

PCB 57 2,3,3',5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 58 2,3,3',5'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 59 2,3,3',6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 60 2,3,4,4'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 61 2,3,4,5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 62 2,3,4,6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 63 2,3,4',5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 64 2,3,4',6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 65 2,3,5,6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 66 2,3',4,4'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 66/80 10 10 10 

PCB 67 2,3',4,5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 68 2,3',4,5'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 69 2,3',4,6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 70 2,3',4',5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 70/76 10 10 10 

PCB 71 2,3',4',6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 72 2,3',5,5'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 73 2,3',5',6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 74 2,4,4',5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 74/61 10 10 10 

PCB 75 2,4,4',6-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 76 2,3',4',5'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 77 3,3',4,4'-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 78 3,3',4,5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 79 3,3',4,5'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 80 3,3',5,5'-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 81 3,4,4',5-Tetrachlorobiphenyl 15 15 15 7 7 

PCB 82 2,2',3,3',4-Pentachlorobiphenyl 15 15 15 7 7 

PCB 83 2,2',3,3',5-Pentachlorobiphenyl 15 15 15 7 7 

PCB 83/108 10 10 10 

PCB 84 2,2',3,3',6-Pentachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 85 2,2',3,4,4'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 85/120 10 10 10 

www.axysanalytical.com Page 40 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 10 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

PCB 86 2,2',3,4,5-Pentachlorobiphenyl 15 15 15 7 7 

PCB 87 2,2',3,4,5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 87/115/116 10 10 10 

PCB 88 2,2',3,4,6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 89 2,2',3,4,6'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 90 2,2',3,4',5-Pentachlorobiphenyl 15 15 15 7 7 

PCB 91 2,2',3,4',6-Pentachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 92 2,2',3,5,5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 93 2,2',3,5,6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 94 2,2',3,5,6'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 95 2,2',3,5',6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 95/93 10 10 10 

PCB 96 2,2',3,6,6'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 97 2,2',3,4',5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 97/86 10 10 10 

PCB 98 2,2',3,4',6'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 99 2,2',4,4',5-Pentachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 100 2,2',4,4',6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 101 2,2',4,5,5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 101/90/89 10 10 10 

PCB 102 2,2',4,5,6'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 103 2,2',4,5',6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 104 2,2',4,6,6'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 105 2,3,3',4,4'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 105/127 10 10 10 

PCB 106 2,3,3',4,5-Pentachlorobiphenyl 15 15 15 7 7 

PCB 107 2,3,3',4',5-Pentachlorobiphenyl 15 15 15 7 7 

PCB 107/109 10 10 10 

PCB 108 2,3,3',4,5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 109 2,3,3',4,6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 110 2,3,3',4',6-Pentachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 111 2,3,3',5,5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 112 2,3,3',5,6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 113 2,3,3',5',6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 114 2,3,4,4',5-Pentachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 115 2,3,4,4',6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 116 2,3,4,5,6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 117 2,3,4',5,6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 118 2,3',4,4',5-Pentachlorobiphenyl 15 15 15 7 7 

PCB 118/116 10 10 10 

PCB 119 2,3',4,4',6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 120 2,3',4,5,5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 121 2,3',4,5',6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 122 2,3,3',4',5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 123 2,3',4,4',5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 124 2,3',4',5,5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 125 2,3',4',5',6-Pentachlorobiphenyl 15 15 15 7 7 

PCB 126 3,3',4,4',5-Pentachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 127 3,3',4,5,5'-Pentachlorobiphenyl 15 15 15 7 7 

PCB 128 2,2',3,3',4,4'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 129 2,2',3,3',4,5-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 130 2,2',3,3',4,5'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 131 2,2',3,3',4,6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 131/142 10 10 10 

www.axysanalytical.com Page 41 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 11 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

PCB 132 2,2',3,3',4,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 133 2,2',3,3',5,5'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 134 2,2',3,3',5,6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 134/143 10 10 10 

PCB 135 2,2',3,3',5,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 136 2,2',3,3',6,6'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 137 2,2',3,4,4',5-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 138 2,2',3,4,4',5'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 138/163/164 10 10 10 

PCB 139 2,2',3,4,4',6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 140 2,2',3,4,4',6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 141 2,2',3,4,5,5'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 142 2,2',3,4,5,6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 143 2,2',3,4,5,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 144 2,2',3,4,5',6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 144/135 10 10 10 

PCB 145 2,2',3,4,6,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 146 2,2',3,4',5,5'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 147 2,2',3,4',5,6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 148 2,2',3,4',5,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 149 2,2',3,4',5',6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 149/139 10 10 10 

PCB 150 2,2',3,4',6,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 151 2,2',3,5,5',6-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 152 2,2',3,5,6,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 153 2,2',4,4',5,5'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 154 2,2',4,4',5,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 155 2,2',4,4',6,6'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 156 2,3,3',4,4',5-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 157 2,3,3',4,4',5'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 158 2,3,3',4,4',6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 158/160 10 10 10 

PCB 159 2,3,3',4,5,5'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 160 2,3,3',4,5,6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 161 2,3,3',4,5',6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 162 2,3,3',4',5,5'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 163 2,3,3',4',5,6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 164 2,3,3',4',5',6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 165 2,3,3',5,5',6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 166 2,3,4,4',5,6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 167 2,3',4,4',5,5'-Hexachlorobiphenyl 15 15 15 7 7 

PCB 168 2,3',4,4',5',6-Hexachlorobiphenyl 15 15 15 7 7 

PCB 169 3,3',4,4',5,5'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 170 2,2',3,3',4,4',5-Heptachlorobiphenyl 15 15 15 7 7 

PCB 170/190 10 10 10 

PCB 171 2,2',3,3',4,4',6-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 172 2,2',3,3',4,5,5'-Heptachlorobiphenyl 15 15 15 7 7 

PCB 172/192 10 10 10 

PCB 173 2,2',3,3',4,5,6-Heptachlorobiphenyl 15 15 15 7 7 

PCB 174 2,2',3,3',4,5,6'-Heptachlorobiphenyl 15 15 15 7 7 

PCB 174/181 10 10 10 

PCB 175 2,2',3,3',4,5',6-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 176 2,2',3,3',4,6,6'-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 177 2,2',3,3',4,5',6'-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

www.axysanalytical.com Page 42 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 12 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

PCB 178 2,2',3,3',5,5',6-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 179 2,2',3,3',5,6,6'-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 180 2,2',3,4,4',5,5'-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 181 2,2',3,4,4',5,6-Heptachlorobiphenyl 15 15 15 7 7 

PCB 182 2,2',3,4,4',5,6'-Heptachlorobiphenyl 15 15 15 7 7 

PCB 183 2,2',3,4,4',5',6-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 184 2,2',3,4,4',6,6'-Heptachlorobiphenyl 15 15 15 7 7 

PCB 185 2,2',3,4,5,5',6-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 186 2,2',3,4,5,6,6'-Heptachlorobiphenyl 15 15 15 7 7 

PCB 187 2,2',3,4',5,5',6-Heptachlorobiphenyl 15 15 15 7 7 

PCB 187/182 10 10 10 

PCB 188 2,2',3,4',5,6,6'-Heptachlorobiphenyl 15 15 15 7 7 

PCB 189 2,3,3',4,4',5,5'-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 190 2,3,3',4,4',5,6-Heptachlorobiphenyl 15 15 15 7 7 

PCB 191 2,3,3',4,4',5',6-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 192 2,3,3',4,5,5',6-Heptachlorobiphenyl 15 15 15 7 7 

PCB 193 2,3,3',4',5,5',6-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 194 2,2',3,3',4,4',5,5'-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 195 2,2',3,3',4,4',5,6-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 196 2,2',3,3',4,4',5,6'-Octachlorobiphenyl 15 15 15 7 7 

PCB 196/203 10 10 10 

PCB 197 2,2',3,3',4,4',6,6'-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 198 2,2',3,3',4,5,5',6-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 199 2,2',3,3',4,5,5',6'-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 200 2,2',3,3',4,5,6,6'-Octachlorobiphenyl 15 15 15 7 7 

PCB 201 2,2',3,3',4,5',6,6'-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 202 2,2',3,3',5,5',6,6'-Octachlorobiphenyl 15 15 15 7 7 

PCB 203 2,2',3,4,4',5,5',6-Octachlorobiphenyl 15 15 15 7 7 

PCB 204 2,2',3,4,4',5,6,6'-Octachlorobiphenyl 15 15 15 7 7 

PCB 205 2,3,3',4,4',5,5',6-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 206 2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 207 2,2',3,3',4,4',5,6,6'-Nonachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 208 2,2',3,3',4,5,5',6,6'-Nonachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

PCB 209 Decachlorobiphenyl 10, 15 10, 15 10, 15 7 7 

Total Monochlorobiphenyls 15 15 15 

Total Dichlorobiphenyls 10, 15 10, 15 10, 15 

Total Trichlorobiphenyls 10, 15 10, 15 10, 15 

Total Tetrachlorobiphenyls 10, 15 10, 15 10, 15 

Total Pentachlorobiphenyls 10, 15 10, 15 10, 15 

Total Hexachlorobiphenyls 10, 15 10, 15 10, 15 

Total Heptachlorobiphenyls 10, 15 10, 15 10, 15 

Total Octachlorobiphenyls 10, 15 10, 15 10, 15 

Total Nonachlorobiphenyls 10, 15 10, 15 10, 15 

Total Decachlorobiphenyls 10 10 10 

Total Polychlorinated biphenyls 10 10 10 7 

 

Aroclors 

Aroclor 1260 10 10 10 7 7 

Aroclor 1254 10 10 10 7 7 

Aroclor 1268 10 10 10 

Aroclor 1221 10 10 10 7 7 

Aroclor 1232 10 10 10 7 7 

Aroclor 1248 10 10 10 7 7 

Aroclor 1016 7 7 

www.axysanalytical.com Page 43 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 13 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

Aroclor 1242 7 7 

Aroclor 1242/1016 10 10 10 

 

Pesticides 

2,4'-DDD 10, 16 10, 16 10, 16 16 

2,4'-DDE 10, 16 10, 16 10, 16 16 

2,4'-DDT 10, 16 10, 16 10, 16 16 

4,4'-DDD 10, 16 10, 16 10, 16 16 

4,4'-DDE 10, 16 10, 16 10, 16 16 

4,4'-DDT 10, 16 10, 16 10, 16 16 

Aldrin 10, 16 10, 16 10, 16 16 

Alpha-HCH 10, 16 10, 16 10, 16 16 

Beta-HCH 10, 16 10, 16 10, 16 16 

cis-Chlordane (alpha-Chlordane) 10, 16 10, 16 10, 16 16 

cis-Nonachlor 10, 16 10, 16 10, 16 16 

Delta-HCH 10, 16 10, 16 10, 16 16 

Dieldrin 10, 16 10, 16 10, 16 16 

Endosulphan I 10, 16 10, 16 10, 16 16 

Endosulphan II 10, 16 10, 16 10, 16 16 

Endosulphan sulphate 10, 16 10, 16 10, 16 16 

Endrin 10, 16 10, 16 10, 16 16 

Endrin aldehyde 10, 16 10, 16 16 16 

Endrin ketone 10, 16 10, 16 10, 16 16 

Gamma-HCH (Lindane) 10, 16 10, 16 10, 16 16 

Heptachlor 10, 16 10, 16 10, 16 16 

Heptachlor epoxide 10, 16 10, 16 10, 16 16 

Hexachlorobenzene 10, 16 10, 16 10, 16 16 

Hexachlorobutadiene 16 16 

Methoxychlor 10, 16 10, 16 10, 16 16 

Mirex 10, 16 10, 16 10, 16 16 

Oxychlordane 10, 16 10, 16 10, 16 16 

Toxaphene 10 10 10 

trans-Chlordane (gamma-Chlordane) 10, 16 10, 16 10, 16 16 

trans-Nonachlor 16 10, 16 10, 16 16 

 

BDE - Brominated Diphenylethers 

BDE 7 2,4-dibromodiphenylether 17 17 17 

BDE 8 2,4’-dibromodiphenylether 17 17 17 

BDE 10 2,6-dibromodiphenylether 17 17 17 

BDE 11 3,3’-dibromodiphenylether 17 17 17 

BDE 12 3,4-dibromodiphenylether 17 17 17 

BDE 13 3,4’-dibromodiphenylether 17 17 17 

BDE 15 4,4’-dibromodiphenylether 17 17 17 

BDE 17 2,2’,4-tribromodiphenylether 17 17 17 

BDE 25 2,3’,4-tribromodiphenylether 17 17 17 

BDE 28 2,4,4’-tribromodiphenylether 17 17 17 

BDE 30 2,4,6-tribromodiphenylether 17 17 17 

BDE-33 2’,3,4-tribromodiphenylether 17 17 17 

BDE 35 3,3’,4-tribromodiphenylether 17 17 17 

BDE 37 3,4,4’-tribromodiphenylether 17 17 17 

BDE 47 2,2’,4,4’-tetrabromodiphenylether 17 17 17 

BDE 49 2,2’,4,5’-tetrabromodiphenylether 17 17 17 

BDE 66 2,3’,4,4’-tetrabromodiphenylether 17 17 17 

BDE 75 2,4,4’,6-tetrabromodiphenylether 17 17 17 

www.axysanalytical.com Page 44 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 14 of 18 

Canadian Association for 

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(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

BDE 77 3,3’,4,4’-tetrabromodiphenylether 17 17 17 

BDE 85 2,2’,3,4,4’-pentabromodiphenylether 17 17 17 

BDE 99 2,2’,4,4’,5-pentabromodiphenylether 17 17 17 

BDE 100 2,2’,4,4’,6-pentabromodiphenylether 17 17 17 

BDE 105 2,3,3’,4,4’-pentabromodiphenylether 17 17 17 

BDE 116 2,3,4,5,6-pentabromodiphenylether 17 17 17 

BDE 119 2,3’,4,4’,6-pentabromodiphenylether 17 17 17 

BDE 126 3,3’,4,4’,5-pentabromodiphenylether 17 17 17 

BDE 140 2,2’,3,4,4’,6’-hexabromodiphenylether 17 17 17 

BDE 153 2,2’,4,4’,5,5’-hexabromodiphenylether 17 17 17 

BDE 154 2,2’,4,4’,5’,6-hexabromodiphenylether 17 17 17 

BDE 155 2,2’,4,4’,6,6’-hexabromodiphenylether 17 17 17 

BDE 166 2,3,4,4’,5,6-hexabromodiphenylether 17 17 17 

BDE 181 2,2’,3,4,4’,5,6-heptabromodiphenylether 17 17 17 

BDE-183 2,2’,3,4,4’,5’,6-heptabromodiphenylether 17 17 17 

BDE 190 2,3,3’,4,4’,5,6-heptabromodiphenylether 17 17 17 

BDE 206 2,2’,3,3’,4,4’,5,5’,6-nonabromodiphenylether 17 17 17 

BDE 207 2,2’,3,3’,4,4’,5,6,6’-nonabromodiphenylether 17 17 17 

BDE 208 2,2’,3,3’,4,5,5’,6,6’-nonabromodiphenylether 17 17 17 

BDE 209 Decabromodiphenylether 17 17 17 

 

PFC – Perfluorinated Organic Compounds 

Perfluorobutanoate (PFBA) 14 12 13 

Perfluoropentanoate (PFPeA) 14 12 13 

Perfluorohexanoate (PFHxA) 14 12 13 

Perfluoroheptanoate (PFHpA) 14 12 13 

Perfluorooctanoate (PFOA) 14 12 13 

Perfluorononanoate (PFNA) 14 12 13 

Perfluorodecanoate (PFDA) 14 12 13 

Perfluoroundecanoate (PFUnA) 14 12 13 

Perfluorododecanoate (PFDoA) 14 12 13 

Perfluorobutanesulfonate (PFBS) 14 12 13 

Perfluorohexanesulfonate (PFHxS) 14 12 13 

Perfluorooctanesulfonate (PFOS) 14 12 13 

Perfluorooctane sulfonamide (PFOSA) 14 12 13 

 

PAH 

Anthracene 18 18 

Pyrene 18 18 

Benzo[ghi]perylene 18 18 

Benzo[e]pyrene 18 18 

Indeno[1,2,3-cd]pyrene 18 18 

Perylene 18 18 

Benzo[b]fluoranthene 18 18 

Fluoranthene 18 18 

Benzo[k]fluoranthene 18 

Acenaphthylene 18 18 

Chrysene 18 18 

Benzo[a]pyrene 18 18 

Dibenz[ah]anthracene 18 18 

Benz[a]anthracene 18 18 

Acenaphthene 18 18 

Phenanthrene 18 18 

Fluorene 18 18 

www.axysanalytical.com Page 45 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 15 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

Naphthalene 18 18 

 

PPCP (Pharmaceutical and Personal Care Products) 

Acetaminophen 19 19 

Azithromycin 19 19 

Caffeine 19 19 

Carbadox 19 19 

Carbamazepine 19 19 

Cefotaxime 19 19 

Ciprofloxacin 19 19 

Clarithromycin 19 19 

Clinafloxacin 19 19 

Cloxacillin 19 19 

Dehydronifedipine 19 19 

Digoxigenin 19 19 

Digoxin 19 19 

Diltiazem 19 19 

1,7-Dimethylxanthine 19 19 

Diphenhydramine 19 19 

Enrofloxacin 19 19 

Erythromycin 19 19 

Flumequine 19 19 

Fluoxetine 19 19 

Lincomycin 19 19 

Lomefloxacin 19 19 

Miconazole 19 19 

Norfloxacin 19 19 

Norgestimate 19 19 

Ofloxacin 19 19 

Ormetoprim 19 19 

Oxacillin 19 19 

Oxolinic acid 19 19 

Penicillin G 19 19 

Penicillin V 19 19 

Roxithromycin 19 19 

Sarafloxacin 19 19 

Sulfachloropyridazine 19 19 

Sulfadiazine 19 19 

Sulfadimethoxine 19 19 

Sulfamerazine 19 19 

Sulfamethazine 19 19 

Sulfamethizole 19 19 

Sulfamethoxazole 19 19 

Sulfanilamide 19 19 

Sulfathiazole 19 19 

Thiabendazole 19 19 

Trimethoprim 19 19 

Tylosin 19 19 

Virginiamycin 19 19 

 

Anhydrochlortetracycline (ACTC) 19 19 

Anhydrotetracycline (ATC) 19 19 

Chlortetracycline (CTC) 19 19 

Demeclocycline 19 19 

www.axysanalytical.com Page 46 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 16 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

Doxycycline 19 19 

4-Epianhydrochlortetracycline (EACTC) 19 19 

4-Epianhydrotetracycline (EATC) 19 19 

4-Epichlortetracycline (ECTC) 19 19 

4-Epioxytetracycline (EOTC) 19 19 

4-Epitetracycline (ETC) 19 19 

Isochlortetracycline (ICTC) 19 19 

Minocycline 19 19 

Oxytetracycline (OTC) 19 19 

Tetracycline (TC) 19 19 

 

Bisphenol A 19 19 

Furosemide 19 19 

Gemfibrozil 19 19 

Glipizide 19 19 

Glyburide 19 19 

Hydrochlorothiazide 19 19 

2-hydroxy-ibuprofen 19 19 

Ibuprofen 19 19 

Naproxen 19 19 

Triclocarban 19 19 

Triclosan 19 19 

Warfarin 19 19 

 

Albuterol 19 19 

Amphetamine 19 19 

Atenolol 19 19 

Atorvastatin 19 19 

Cimetidine 19 19 

Clonidine 19 19 

Codeine 19 19 

Cotinine 19 19 

Enalapril 19 19 

Hydrocodone 19 19 

Metformin 19 19 

Oxycodone 19 19 

Ranitidine 19 19 

Triamterene 19 19 

 

Alprazolam 19 19 

Amitriptyline 19 19 

Amlodipine 19 19 

Benzoylecgonine 19 19 

Benztropine 19 19 

Betamethasone 19 19 

Cocaine 19 19 

DEET (N,N-diethyl-m-toluamide) 19 19 

Desmethyldiltiazem 19 19 

Diazepam 19 19 

Fluocinonide 19 19 

Fluticasone propionate 19 19 

Hydrocortisone 19 19 

10-hydroxy-amitriptyline 19 19 

Meprobamate 19 19 

www.axysanalytical.com Page 47 of 49
AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 17 of 18 

Canadian Association for 

Laboratory Accreditation 

(CALA)

Washington 

State 

Department 

of Ecology

Accreditation No.: 

A 2637 Lab. ID: C404

TABLE 2

W S Pulp T NP 

W S

Methylprednisolone 19 19 

Metoprolol 19 19 

Norfluoxetine 19 19 

Norverapamil 19 19 

Paroxetine 19 19 

Prednisolone 19 19 

Prednisone 19 19 

Promethazine 19 19 

Propoxyphene 19 19 

Propranolol 19 19 

Sertraline 19 19 

Simvastatin 19 19 

Theophylline 19 19 

Trenbolone 19 19 

Trenbolone acetate 19 19 

Valsartan 19 19 

Verapamil 19 19 

Table 1 and Table 2 - Explanation of Terms Used: 

• NELAP = National Environmental Laboratory Accreditation Program 

• Non-potable water = water not fit for consumption without treatment as it may contain 

pollutants, contaminants, minerals or infective agents. Surface water, ground water, rainwater, 

effluents as well as any other non-drinking water sources are included in this category. 

• Solid = environmental solid sample. Soil, sediment, biosolids, hazardous waste, mixed phase 

samples with significant solids content are included in this category. 

• Performance based implementation = methodology follows that of the method reference but 

modifications deemed by AXYS as minor 1 may apply, results meet method reference data 

quality standard. 

• Performance based modification = modifications deemed by AXYS as significant2

 have been 

made to method reference protocol, results meet method reference accuracy standard. The 

suitability of the methodology for any method prescriptive applications should be assessed 

based on the modifications made and the specific work requirements. 

• Performance based method = an in-house AXYS method, published method reference not 

applicable. 

• GC/LRMS = gas chromatography, low resolution mass spectrometry detection. 

• GC/HRMS = gas chromatography, high resolution mass spectrometry detection. 

• GC/ECD = gas chromatography, electron capture detection. 

• LC/MS-MS = liquid chromatography, mass spectrometry-mass spectrometry detection. 

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AXYS Analytical Services Ltd. 

ACC-101 Rev 06, 29-Jun-2011 Page 18 of 18 

Note 1: 

Performance Based Implementation - Examples of Minor Modifications 

- use of additional isotopically labeled references 

- adjustment of calibration range 

- adjustment of clean-up technique 

- use of a different extraction of same general type (example soxhlet vs soxhlet Dean Stark) 

- addition of matrix type using same principles (example addition of tissue matrix using same 

detection principle and similar extraction type) 

Note 2: 

Performance Based Modification - Examples of Significant Modifications 

- different acquisition conditions using same detection principle (example MS SIM vs. full scan) 

- different internal control limits while meeting method reference accuracy standard 

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